CN114197210A - Hydrophobically modified viscose fiber and preparation method thereof - Google Patents

Hydrophobically modified viscose fiber and preparation method thereof Download PDF

Info

Publication number
CN114197210A
CN114197210A CN202111567669.5A CN202111567669A CN114197210A CN 114197210 A CN114197210 A CN 114197210A CN 202111567669 A CN202111567669 A CN 202111567669A CN 114197210 A CN114197210 A CN 114197210A
Authority
CN
China
Prior art keywords
fiber
viscose
spinning
washing
mixing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111567669.5A
Other languages
Chinese (zh)
Other versions
CN114197210B (en
Inventor
林庆辉
解晴晴
黄志冰
黄帛彦
郑超
吴晓东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sateri Fujian Fiber Co ltd
Original Assignee
Sateri Fujian Fiber Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sateri Fujian Fiber Co ltd filed Critical Sateri Fujian Fiber Co ltd
Priority to CN202111567669.5A priority Critical patent/CN114197210B/en
Publication of CN114197210A publication Critical patent/CN114197210A/en
Application granted granted Critical
Publication of CN114197210B publication Critical patent/CN114197210B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath
    • D01F2/10Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/395Isocyanates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties

Abstract

The invention discloses a hydrophobic modified viscose fiber and a preparation method thereof, wherein needle wood dissolving pulp and broad leaf wood dissolving pulp mixed pulp with whiteness of more than 89% and methyl fiber content of more than 90% are selected, viscose spinning stock solution is prepared after a series of treatments, and the viscose spinning stock solution is uniformly mixed with titanium dioxide dispersion liquid and then is sent to spinning. The spinning solution is sent to a spinning machine to react, solidify and regenerate nascent fiber; drafting, orienting and cutting the solidified and regenerated nascent fiber, and then feeding the nascent fiber into a fluff tank to form viscose staple fiber fluff with uniform fiber layer thickness; and (3) delivering the viscose staple fiber from the fluff tank into a refiner, performing hydrophobic modification on the fiber surface in a refining oiling process, and drying to obtain the hydrophobically modified viscose fiber. The hydrophobic viscose fiber prepared by the invention has good hydrophobic performance and washability. In the preparation process, the problems of agglomeration generated by mixing a water repellent agent and an oil agent, the washability of the hydrophobic modified fiber and the spinnability generated by an addition method before spinning are effectively solved.

Description

Hydrophobically modified viscose fiber and preparation method thereof
Technical Field
The invention relates to the technical field of chemical fiber processing, in particular to a preparation method of hydrophobically modified viscose fiber and the hydrophobically modified viscose fiber prepared by the preparation method.
Background
With the improvement of economic living standard and the increase of population, people have more and more demands on the non-woven fabrics for medical sanitary materials. The clean high-whiteness viscose fibers are a type of differential viscose fibers and are widely used in the field of non-woven fabrics, but when the clean high-whiteness viscose fibers are used as surface layer materials in the field of paper diapers, the surface layer materials are easy to diffuse liquid quickly to generate a liquid reverse osmosis phenomenon due to poor hydrophobic performance (the water absorption and sedimentation time is usually less than 5 s), and the wearing comfort of the paper diapers is poor. In the field of paper diapers, in order to avoid the phenomenon of liquid reverse osmosis, a low-water-absorption material is often used as a surface layer material, but the wearing comfort is poor, and the diaper is not a biodegradable material. Therefore, in order to solve the above problems, it is necessary to develop hydrophobically modified viscose fibers to meet the market demand.
The construction of a hydrophobic coating on the surface of a fiber by an after-finishing method is one of the main methods for preparing hydrophobic fiber materials. CN201910871468.0 discloses a hydrophobic modification method of fiber, which adopts a mode of spraying a hydrophobic agent to carry out hydrophobic modification on the fiber. CN201510158836.9 discloses a method for preparing a super-hydrophobic textile by fiber surface polymerization modification, which grafts a methacrylate monomer onto a polyester surface by a surface-initiated atom transfer radical polymerization (SI-ATRP) method to form a high polymer hydrophobic layer on the fiber surface, thereby obtaining a super-hydrophobic polyester fabric. CN201510913731.X discloses a fluorine-free super-hydrophobic cotton fabric and a preparation method thereof, wherein hydroxyl of cotton fiber and nano TiO are utilized in the method2The chemical reaction between hydroxyl groups in the hydrosol enables the constructed rough surface to have good fastness, and the structural characteristics of the bionic lotus leaf surface are adopted, and the molten wax is solidified and crystallized on the rough surface of the oxide to carry out organic modification, so that the prepared fabric has excellent stability in the super-hydrophobic property. CN200910053646.5 discloses a fluorine-free nano durable super-water-repellent finishing method for cellulose fabrics, and relates to a method for preparing super-water-repellent textiles by utilizing a sol-gel technology. CN201880082162.0 discloses a method for producing a finely-divided hydrophobically modified cellulose fiber, which comprises a step of finely-dividing a hydrophobically modified cellulose fiber having a specific average fiber length in an organic solvent.
Although the existing hydrophobic fiber preparation technology makes certain progress, in the industrial production of water repellent finishing of cellulose fibers, because the fibers are required to be soaked in the water repellent finishing agent for tens of seconds to obtain the water repellent effect, some water repellent finishing agents which need to be soaked for a long time to have the water repellent effect are not suitable. In addition, the problems of poor fiber hydrophobic property uniformity, washability resistance, high cost, poor finished product quality and the like still exist in the preparation of the hydrophobically modified viscose fiber.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the preparation method of the hydrophobically modified viscose fiber is provided.
In order to solve the problems, the specific technical scheme of the invention is as follows:
a hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 4-6 g/L of oil agent component, 0.3-0.5 g/L of hydrogen peroxide and acid into water at the temperature of 68-72 ℃ to prepare an oil bath with the pH value of 3-4; and (3) continuously adding the dispersing agent in the oil bath, mixing for 5-15 min, then adding the fluorine-free hydrophobic agent, mixing for 5-15 min, finally adding the bridging agent, and mixing for 5-10 min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl cellulose content of more than 90%, and mixing the raw materials according to the weight ratio of 6-7: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100-0.9: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the viscose fiber.
Further, in the oiling and water repellent finishing liquid in the step (1), the ionic property of the oil agent is anion, the water repellent agent is a polyurethane compound, and the mass concentration of the water repellent agent in the oil bath is 0.4-2.0%; the dispersant is a nonionic surfactant; the bridging agent is isocyanate, and the mass ratio of the bridging agent to the hydrophobic agent is 1: 4-1: 6.
further, the addition method of each auxiliary agent in the oil bath comprises the following steps: and (3) in an oil bath, firstly adding a dispersing agent, mixing for 5-15 min, then adding a fluorine-free hydrophobic agent, mixing for 5-15 min, then adding a bridging agent, and mixing for 5-10 min for later use.
Further, the dispersant in the step (1) is polyoxyethylene derivative.
Further, the ionic nature of the hydrophobic agent in the step (1) is cation.
Further, the ionic property of the bridging agent in the step (1) is nonionic.
Further, in the dissolving process in the step (2), adding a fatty amine polyoxyethylene ether denaturant, wherein the mass ratio of the denaturant to the pulp is (2-4): 10000;
further, the coagulating bath in the step (2) comprises 110-120 g/L sulfuric acid, 300-320 g/L sodium sulfate, 9-13 g/L zinc sulfate and 10-11 g/L Berol Spin653 surfactant;
further, the spinning speed of the spinning machine in the step (2) is 55-60 m/min.
Further, the temperature of the first water washing in the step (3) is 70-75 ℃, the temperature of the second water washing is 60-70 ℃, the temperature of the third water washing is 55-70 ℃, and the temperature of the final water washing is 70-75 ℃.
Further, the desulfurizing agent used in the desulfurizing process in the step (3) is one or two of sodium hydroxide and sodium sulfide, the concentration of the desulfurizing agent is 2-4 g/L, and the desulfurizing temperature is 70-80 ℃.
Further, the temperature of the drying in the step (3) is 130-145 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.65-1.75 dtex; the length is 38-40 mm; the dry breaking strength is more than or equal to 1.7 cN/dtex; the dry breaking elongation is 18.0-25.0%; the whiteness is more than or equal to 85.0 percent; the water absorption settling time is more than or equal to 20 s.
The detection method of the index can refer to the industry standard FZT 54032-2010 clean high-whiteness viscose staple fiber.
The invention optimizes the spinning speed to obtain proper post-processing time and ensure the balance of yield and quality index.
The dispersant adopted by the invention is a nonionic surfactant, has better dispersing and anti-precipitation effects, and prevents precipitates from appearing in the oil and water repellent finishing liquid.
The ionic property of the hydrophobic agent adopted by the invention is cation, so that the hydrophobic property of the fiber is improved.
The invention adopts isocyanate bridging agent to improve the washability of the hydrophobic property of the fiber.
The invention selects proper concentration of the hydrophobic agent to reduce the reduction of the mechanical property and whiteness of the fiber caused by excessively high content of the hydrophobic agent.
The invention selects proper drying temperature to ensure that the hydrophobic performance has washability and avoid the yellowing phenomenon of hydrophobic fiber caused by overhigh temperature in drying.
The invention has the beneficial effects that:
(1) the polyurethane hydrophobic agent is preferably selected in the invention, and the prepared hydrophobic viscose fiber has better hydrophobic property and certain washability, and can be used in the fields of textile and non-woven.
(2) The invention adopts the mode of adding the dispersant and then adding the hydrophobic agent, thereby avoiding the problem of agglomeration generated by mixing the hydrophobic agent and the oil agent.
(3) The invention selects proper bridging agent to improve the hydrophobic property and wash resistance of the fiber.
(4) The invention preferably selects a cationic fluorine-free hydrophobic agent which has small influence on the whiteness of the fiber, and introduces the cationic fluorine-free hydrophobic agent to the fiber by adopting a post-treatment method, thereby being beneficial to avoiding the spinnability problem caused by the addition method before spinning and the waste liquid treatment problem caused by the loss of the hydrophobic agent in the spinning process.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Example 1
A hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 4g/L of oil agent component, 0.3g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 68 ℃ to prepare an oil bath with the pH value of 3; and continuously adding 1g/L fatty alcohol-polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 5min, adding 4g/L cationic polyurethane resin serving as a hydrophobic agent, mixing for 5min, finally adding 1g/L nonionic isocyanate serving as a bridging agent, and mixing for 5min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl fiber content of more than 90%, and mixing the raw materials in a ratio of 6: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
The parameters that are preferred are those that,
preferably, the oil agent in step (1) has an anionic property.
Preferably, the ionic nature of the hydrophobic agent described in step (1) is cationic.
In the step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 2: 10000;
the coagulating bath comprises 110g/L sulfuric acid, 300g/L sodium sulfate, 9g/L zinc sulfate and 10g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 55 m/min.
The temperature of the first washing in the step (3) is 70 ℃, the temperature of the second washing is 60 ℃, the temperature of the third washing is 55 ℃, and the temperature of the final washing is 70 ℃.
The desulfurizer used in the desulfurization process in the step (3) is sodium hydroxide, the concentration of the desulfurizer is 2g/L, and the desulfurization temperature is 70 ℃.
The drying temperature in the step (3) is 130 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.65 dtex; the length is 38 mm; dry breaking strength 1.7 cN/dtex; the dry elongation at break was 25.0%; the whiteness is 86.0 percent; the water absorption settling time is 20 s.
Example 2
A hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 3g/L of oil agent component, 0.5g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 72 ℃ to prepare an oil bath with the pH value of 4; and continuously adding 2g/L fatty alcohol-polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 15min, then adding 5g/L cationic polyurethane modified organosilicon hydrophobic agent, mixing for 15min, finally adding 1g/L nonionic isocyanate serving as a bridging agent, and mixing for 15min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl cellulose content of more than 90%, and mixing the raw materials in a proportion of 7: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.9: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
The parameters that are preferred are those that,
in the step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 4: 10000;
the coagulating bath comprises 120g/L sulfuric acid, 320g/L sodium sulfate, 13g/L zinc sulfate and 11g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 60 m/min.
The temperature of the first water washing in the step (3) is 75 ℃, the temperature of the second water washing is 70 ℃, the temperature of the third water washing is 70 ℃, and the temperature of the final water washing is 75 ℃.
The desulfurizing agents used in the desulfurizing process in the step (3) are 3g/L sodium hydroxide and 1g/L sodium sulfide, and the desulfurizing temperature is 80 ℃.
The drying temperature in the step (3) is 145 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.75 dtex; the length is 40 mm; dry breaking strength 2.2 cN/dtex; the dry elongation at break was 18.0%; the whiteness is 85.0 percent; the water absorption settling time is 120 s.
Example 3
A hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 3.5g/L of oil agent component, 0.4g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 70 ℃ to prepare an oil bath with the pH value of 3.5; and continuously adding 1g/L fatty alcohol-polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 10min, then adding 5g/L cationic polyurethane modified organosilicon hydrophobic agent, mixing for 10min, finally adding 1g/L nonionic isocyanate bridging agent, and mixing for 10min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl fiber content of more than 90%, and mixing the raw materials in a ratio of 6: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
Preferred parameters, in step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 4: 10000;
the coagulating bath comprises 115g/L sulfuric acid, 300g/L sodium sulfate, 13g/L zinc sulfate and 11g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 59 m/min.
The temperature of the first water washing in the step (3) is 75 ℃, the temperature of the second water washing is 70 ℃, the temperature of the third water washing is 55 ℃, and the temperature of the final water washing is 75 ℃.
The desulfurizer used in the desulfurization process in the step (3) is 3g/L of sodium hydroxide, the concentration of the desulfurizer is 3g/L, and the desulfurization temperature is 80 ℃.
The drying temperature in the step (3) is 140 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.70 dtex; the length is 40 mm; dry breaking strength 2.1 cN/dtex; dry elongation at break 22%; the whiteness is 86.0 percent; the water absorption settling time is 180 s.
Example 4
A hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 3.5g/L of oil agent component, 0.4g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 70 ℃ to prepare an oil bath with the pH value of 3.5; and continuously adding 2g/L of octyl phenol polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 10min, then adding 15g/L of cationic polyurethane modified organosilicon hydrophobic agent, mixing for 10min, finally adding 1g/L of nonionic isocyanate bridging agent, and mixing for 10min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl fiber content of more than 90%, and mixing the raw materials in a ratio of 6: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
Preferred parameters, in step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 4: 10000; the coagulating bath comprises 115g/L sulfuric acid, 300g/L sodium sulfate, 13g/L zinc sulfate and 11g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 59 m/min.
The temperature of the first water washing in the step (3) is 75 ℃, the temperature of the second water washing is 70 ℃, the temperature of the third water washing is 55 ℃, and the temperature of the final water washing is 75 ℃.
The desulfurizer used in the desulfurization process in the step (3) is 3g/L of sodium hydroxide, the concentration of the desulfurizer is 3g/L, and the desulfurization temperature is 80 ℃.
The drying temperature in the step (3) is 140 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.70 dtex; the length is 40 mm; dry breaking strength 2.1 cN/dtex; dry elongation at break 22%; the whiteness is 85.0 percent; the water absorption settling time is more than 300 s.
Comparative example 1
A hydrophobically modified viscose fiber and a preparation method thereof comprise the following steps:
(1) preparing oiling water-repellent finishing liquid:
adding 3.5g/L of oil agent component, 0.4g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 70 ℃ to prepare an oil bath with the pH value of 3.5; and continuously adding 1g/L fatty alcohol-polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 10min, then adding 5g/L acrylate hydrophobic agent, mixing for 10min, finally adding 1g/L nonionic isocyanate bridging agent, and mixing for 10min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl fiber content of more than 90%, and mixing the raw materials in a ratio of 6: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
Preferred parameters, in step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 4: 10000;
the coagulating bath comprises 115g/L sulfuric acid, 300g/L sodium sulfate, 13g/L zinc sulfate and 11g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 59 m/min.
The temperature of the first water washing in the step (3) is 75 ℃, the temperature of the second water washing is 70 ℃, the temperature of the third water washing is 55 ℃, and the temperature of the final water washing is 75 ℃.
The desulfurizer used in the desulfurization process in the step (3) is 3g/L of sodium hydroxide, the concentration of the desulfurizer is 3g/L, and the desulfurization temperature is 80 ℃.
The drying temperature in the step (3) is 140 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.70 dtex; the length is 40 mm; dry breaking strength 2.1 cN/dtex; dry elongation at break 22%; the whiteness is 84.0%; the water absorption settling time is 170 s.
As can be seen from the above example 3 and comparative example 1, the whiteness index and the hydrophobic property of the fiber are changed by changing the kind of the hydrophobic agent.
Comparative example 2
(1) Preparing oiling water-repellent finishing liquid:
adding 3.5g/L of oil agent component, 0.4g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 70 ℃ to prepare an oil bath with the pH value of 3.5; and continuously adding 1g/L fatty alcohol-polyoxyethylene ether serving as a dispersing agent in an oil bath, mixing for 10min, then adding 5g/L cationic polyurethane modified organosilicon hydrophobic agent, and mixing for 10min for later use.
(2) Preparing viscose fibers:
selecting softwood dissolving pulp and hardwood dissolving pulp with whiteness of more than 89% and methyl fiber content of more than 90%, and mixing the raw materials in a ratio of 6: mixing the materials according to the mass ratio of 100, then sequentially carrying out the steps of dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening to prepare a viscose spinning solution, uniformly mixing the viscose spinning solution with a titanium dioxide dispersion solution, and then sending the viscose spinning solution into a spinning machine; the mass ratio of the titanium dioxide to the methyl fiber in the viscose stock solution is 0.7: 100. the spinning solution is sent to a spinning machine, sprayed out from a spinneret through a metering pump, and reacts with a coagulating bath in an acid bath tank to coagulate and regenerate nascent fiber; drafting and orienting the solidified and regenerated nascent fiber to form fiber with certain strength, cutting the fiber, and feeding the fiber into a fluff tank; the steam bubbles sprayed from the small holes of the steam spraying pipe at the bottom of the fluff slot disperse the fibers to make the thickness of the fiber layer uniform;
(3) post-treatment of viscose fibers:
and (3) delivering the viscose staple fiber from the fluff tank into a refiner, and sequentially performing primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oiling and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber.
Preferred parameters, in step (2):
in the dissolving process, a fatty amine polyoxyethylene ether denaturant is added, and the mass ratio of the denaturant to the pulp is 4: 10000; the coagulating bath comprises 115g/L sulfuric acid, 300g/L sodium sulfate, 13g/L zinc sulfate and 11g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 59 m/min.
The temperature of the first water washing in the step (3) is 75 ℃, the temperature of the second water washing is 70 ℃, the temperature of the third water washing is 55 ℃, and the temperature of the final water washing is 75 ℃.
The desulfurizer used in the desulfurization process in the step (3) is 3g/L of sodium hydroxide, the concentration of the desulfurizer is 3g/L, and the desulfurization temperature is 80 ℃.
The drying temperature in the step (3) is 140 ℃.
The technical parameters of the hydrophobically modified viscose fiber obtained by the invention are as follows: the fineness is 1.70 dtex; the length is 40 mm; dry breaking strength 2.1 cN/dtex; dry elongation at break 22%; the whiteness is 85.0 percent; the water absorption settling time is 90 s.
As can be seen from the above example 3 and comparative example 2, the hydrophobic properties of the fibers are somewhat reduced without the addition of the bridging agent.

Claims (9)

1. A method of making hydrophobically modified viscose comprising:
the mass ratio of the softwood dissolving pulp to the hardwood dissolving pulp is 6-7: 100, mixing dregs, and preparing a viscose spinning solution by sequentially dipping, squeezing, crushing, ageing, yellowing, dissolving and ripening;
uniformly mixing the viscose spinning solution and the titanium dioxide dispersion solution, feeding the mixture into a spinning machine, spraying the mixture from a spinneret through a metering pump, and reacting the mixture with a coagulating bath in an acid bath tank to obtain nascent fibers;
drafting, orienting and cutting the nascent fiber, and then feeding the nascent fiber into a fluff tank to form viscose staple fiber fluff with uniform fiber layer thickness;
sending the viscose staple fiber into a refiner, and sequentially carrying out primary washing, desulfurization, secondary washing, bleaching, tertiary washing, final washing, oil and water repellent finishing, dehydration and drying to obtain the hydrophobically modified viscose fiber;
wherein: the titer of the hydrophobically modified viscose fiber is 1.65-1.75 dtex; the length is 38-40 mm; the dry breaking strength is more than or equal to 1.7 cN/dtex; the dry breaking elongation is 18.0-25.0%; the whiteness is more than or equal to 85.0 percent; the water absorption settling time is more than or equal to 20 s.
2. The production method according to claim 1, wherein:
the whiteness of the dissolving pulp of the softwood dissolving pulp and the dissolving pulp of the hardwood dissolving pulp are both more than or equal to 89%, and the content of methyl cellulose is both more than or equal to 90%.
3. The production method according to claim 1, wherein:
in the dissolving process, adding a fatty amine polyoxyethylene ether denaturant, wherein the mass ratio of the denaturant to the mixed pulp is (2-4): 10000.
4. the production method according to claim 1, wherein:
the mass ratio of the titanium dioxide to the methyl cellulose in the viscose stock solution is (0.7-0.9): 100.
5. The production method according to claim 1, wherein:
the coagulating bath comprises 110-120 g/L sulfuric acid, 300-320 g/L sodium sulfate, 9-13 g/L zinc sulfate and 10-11 g/L Berol Spin653 surfactant;
the spinning speed of the spinning machine is 50-60 m/min.
6. The production method according to claim 1, wherein:
the first washing temperature is 70-75 ℃, the second washing temperature is 60-70 ℃, the third washing temperature is 55-70 ℃, and the final washing temperature is 70-75 ℃;
the desulfurizer used for desulfurization is one or two of sodium hydroxide and sodium sulfide, the concentration of the desulfurizer is 2-4 g/L, and the desulfurization temperature is 70-80 ℃.
7. The production method according to claim 1, wherein:
the oiling water-repellent finishing liquid is prepared by the following method:
adding 4-6 g/L of oil agent component, 0.3-0.5 g/L of hydrogen peroxide and sulfuric acid into water at the temperature of 68-72 ℃ to prepare an oil bath with the pH value of 3-4;
continuously adding 1-2 g/L of nonionic surfactant serving as a dispersing agent in an oil bath, mixing for 5-15 min, then adding 5-15 g/L of fluorine-free hydrophobic agent, and mixing for 5-15 min;
and finally, adding 1g/L of nonionic bridging agent, and mixing for 5-10 min to obtain the oiling water-repellent finishing liquid.
8. The production method according to claim 1, wherein:
the drying temperature is 130-145 ℃.
9. A hydrophobically modified viscose fiber prepared by the preparation method of any one of claims 1 to 8.
CN202111567669.5A 2021-12-21 2021-12-21 Hydrophobically modified viscose fiber and preparation method thereof Active CN114197210B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111567669.5A CN114197210B (en) 2021-12-21 2021-12-21 Hydrophobically modified viscose fiber and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111567669.5A CN114197210B (en) 2021-12-21 2021-12-21 Hydrophobically modified viscose fiber and preparation method thereof

Publications (2)

Publication Number Publication Date
CN114197210A true CN114197210A (en) 2022-03-18
CN114197210B CN114197210B (en) 2024-03-19

Family

ID=80655570

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111567669.5A Active CN114197210B (en) 2021-12-21 2021-12-21 Hydrophobically modified viscose fiber and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114197210B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107429478A (en) * 2015-03-16 2017-12-01 Cthr·拜特利希有限公司 Floride-free silicic acid anhydride
CN108588880A (en) * 2018-05-15 2018-09-28 赛得利(福建)纤维有限公司 A kind of preparation method of clean high white viscose rayon
JP2019065443A (en) * 2017-10-02 2019-04-25 ダイワボウホールディングス株式会社 Water repellent recycled cellulose fiber, manufacturing method therefor and fiber structure containing the same
CN109930225A (en) * 2019-02-20 2019-06-25 赛得利(福建)纤维有限公司 White viscose rayon of a kind of no chlorine drift height and preparation method thereof
CN110565384A (en) * 2019-07-31 2019-12-13 曹运福 Preparation method of special oiling agent for vortex spun-bonded adhesive fiber
CN112553705A (en) * 2020-12-09 2021-03-26 赛得利(福建)纤维有限公司 Preparation method of flame-retardant viscose fibers

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107429478A (en) * 2015-03-16 2017-12-01 Cthr·拜特利希有限公司 Floride-free silicic acid anhydride
JP2019065443A (en) * 2017-10-02 2019-04-25 ダイワボウホールディングス株式会社 Water repellent recycled cellulose fiber, manufacturing method therefor and fiber structure containing the same
CN108588880A (en) * 2018-05-15 2018-09-28 赛得利(福建)纤维有限公司 A kind of preparation method of clean high white viscose rayon
CN109930225A (en) * 2019-02-20 2019-06-25 赛得利(福建)纤维有限公司 White viscose rayon of a kind of no chlorine drift height and preparation method thereof
CN110565384A (en) * 2019-07-31 2019-12-13 曹运福 Preparation method of special oiling agent for vortex spun-bonded adhesive fiber
CN112553705A (en) * 2020-12-09 2021-03-26 赛得利(福建)纤维有限公司 Preparation method of flame-retardant viscose fibers

Also Published As

Publication number Publication date
CN114197210B (en) 2024-03-19

Similar Documents

Publication Publication Date Title
CN102965751B (en) High-wet-modulus and flame-retardant regenerated cellulose fibers and preparation method thereof
CN109930225B (en) Chlorine-bleaching-free high-whiteness viscose fiber and preparation method thereof
CN108588880B (en) Preparation method of clean high-whiteness viscose fiber
CN101851804B (en) Method for producing fire-retardant anti-melt viscose fibers
CN108677273B (en) Preparation method of fine denier strong viscose fiber
CN104911726B (en) A kind of high-strength flatness viscose rayon of delustring superfine type and preparation method thereof
WO2010132151A2 (en) Fibrillated blend of lyocell and cellulosic low dp pulp
CN110952159B (en) Application of silk fibroin solution in preparation of regenerated cellulose fibers
CN101117737A (en) Bamboo pupa protein fiber long-short yarn and method for making same
CN113638069B (en) Long-carbon-prepared composite modified nano platinum bamboo pulp fiber for mask base cloth and preparation method thereof
DE60123377T2 (en) METHOD FOR PRODUCING FIBERS, FILMS AND OTHER PRODUCTS FROM MODIFIED SOLUBLE CELLULOSE
CN104846453B (en) A kind of superfine type viscose rayon and preparation method thereof
CN109610026A (en) One kind regenerated celulose fibre containing essential oil and preparation method thereof
CN106591991A (en) Production method of bamboo joint type hollow bamboo viscose fibers
CN104862802B (en) A kind of process for preparing high-strength flatness viscose rayon
CN114197210B (en) Hydrophobically modified viscose fiber and preparation method thereof
CN106498527A (en) A kind of process for producing high-wet-modulus fibre cellulose fiber
CN112575402B (en) Preparation method of low-odor viscose fibers
CN112708954B (en) Rose plant extract cellulose fiber and preparation method thereof
CN104831390A (en) Luminous high-strength low-elongation viscose and production method thereof
CN112813517A (en) Method for refining and post-treating nonwoven cellulose fibers and nonwoven cellulose fibers
CN104846455B (en) A kind of high-strength flatness viscose rayon and its preparation method and application
CN104894670B (en) A kind of high tenacity viscose fiber and its preparation method and application
CN109280987B (en) Method for preparing modal fiber from bamboo raw material
CN101130884A (en) Method for preparing viscose fiber using cotton stalk

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant